Deficient Analysis Method for I-131 in

Environmental Water Samples:

The Importance of Rigorous Quality
Control

Greg Barley-Progress Energy

 Success does not consist
in never making mistakes,
but in never making the
same one a second time.
George Bernard Shaw
 NUREG 1301, 1302
I-131 LLDs

 1 pCi/L drinking water

 15 pCi/L if no drinking water pathway
 Originally published in 1979 Branch Technical
Position (BTP) for Regulatory Guide 4.8
 Progress Energy Corporate
Radiochemistry Laboratory
 Part 50 Composite Analyses for HTDs
 Entire fleet
 REMP
 Sample collection for Shearon Harris Plant
 Analyses and REOR preparation for
Progress Energy Carolina plants
 REMP I-131 Test Methods
 Drinking Water Pathway
 I-131 separation onto resin, then analyze
resin by gamma spectroscopy
 Non-Drinking Water Pathway (previous
method)
 Concentrate gamma emitters by heated
evaporation
 1 liter to 500 mL for brackish water
 1 liter to 50 mL for non-brackish water
 History of Evaporation Method
 Developed as a means to minimize
counting time circa 1976
 Developed “in-house” by technically
respected personnel
 Emphasis was on achieving low levels for
I-131 in drinking water
 Evaporation method not evaluated when
BTP and subsequent NUREGs published.
 Back to Basics

 What happens to iodine when it is heated?

 How does one ensure that an analytical
method produces precise, reproducible
results?
 The Problem’s History
 Past quality control blind crosscheck analyses had
not tested the evaporation method for non-drinking
water samples; only the drinking water separation
method had been tested
 There was no central facility procedure or document
containing the Radiochemistry QA elements
 The need to test all methods was not captured in any
facility procedure or document
The Problem Becomes Apparent
 Lab personnel begin testing blind QC crosschecks by
heated evaporation
 Non-volatile nuclides usually in agreement
 Initially the idea that I-131 could volatilize was
recognized, so QCs were analyzed for I-131 prior to
heated evaporation, but missed the connection to
field sample analyses
 During subsequent staff discussions, questions arose
as to why the QCs were being prepared differently for
I-131 analyses than field samples were prepared
 The Problem Unveiled

 Examined the I-131 in QC samples that had

been subjected to heated evaporation
 Where gentle heating was applied, losses were
low (0-10%)
 Where heating was more aggressive, losses were
substantial (0-50%)
 Significance
 Historically, plant I-131 not found in these
non-drinking water samples
 However, the requirement to meet the LLD of
15 pCi/L was not met for some number of
samples that were subjected to aggressive
heating
 Problem potentially dates back to initial
development of the method in mid-1970’s
 Causes
 No central QA/QC document or procedure that set
forth the required programmatic elements
 QA/QC Program failed to change to meet changing
regulatory requirements (BTP, NUREGs)
 Insufficient priority assigned to QA/QC Program by
supervision
 No analytical standard for method
 Overconfidence in the method
 Corrective Actions
 Discontinue heated evaporation
 Direct gamma analyses without evaporation,
except for drinking water separation onto resin
 Review other test methods to ensure all have
some QC verification
 Develop central QA/QC procedure
 Increased resource and priority on QA/QC
Program
 Summary
 Ensure that all analytical methods are
tested by some quality control measure
 Always exercise questioning attitude
 Just because a method was developed by
respected individuals and has been in use
for a long time does not necessarily make
it correct
 When there are questions, keep going until
they are answered acceptably
Questions, comments?